CN102391942B - The method processing fluid particularly beverage - Google Patents
The method processing fluid particularly beverage Download PDFInfo
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- CN102391942B CN102391942B CN201110294359.0A CN201110294359A CN102391942B CN 102391942 B CN102391942 B CN 102391942B CN 201110294359 A CN201110294359 A CN 201110294359A CN 102391942 B CN102391942 B CN 102391942B
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- sedimentary
- fluid
- granular materials
- filter cylinder
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
- C12H1/04—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
- C12H1/0416—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material
- C12H1/0424—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material with the aid of a polymer
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/42—Preservation of non-alcoholic beverages
- A23L2/46—Preservation of non-alcoholic beverages by heating
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
- A23L2/72—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
- A23L2/80—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by adsorption
Abstract
Be there is the granular materials of the sedimentary form in upstream side and downstream by use, one is provided to be used for processing fluid, particularly beverage such as medicated beer, wine or the method for fruit juice, wherein guides described fluid stream to cause downstream in the first temperature from the upstream side of described sedimentary.The time period processed to extend described granular materials can be used for, it is proposed that regulate described sedimentary again, then carrying out the process again of described fluid, wherein said regulation again includes that sedimentary is heated to the second temperature by step；With sedimentary is cooled to the 3rd temperature, average cooldown rate is in the range of a maximum of about of 20 DEG C/min.
Description
Background of invention
The present invention relates to a kind of method processing fluid, particularly beverage, more specifically medicated beer.
The fluid including beverage is processed for various purposes.At the beverage such as medicated beer, wine or fruit juice
In preparation, so-called stabilization process is needs, and this technique at least significantly reduces in fluid storage and fortune
Defeated period fluid may cause the amount of the component of the generation of flocculation or mist.Filter and absorption is institute for this purpose
The most important mechanism used.Other fluid is required for following aspect and processes, such as, and suspended solid
Removal, other chemical reaction to be carried out.
Generally, the sedimentary of granular materials is used to carry out such process, and such sedimentary can be with filter cake
Form use.
Granular materials is deposited in filtration cartridges in fluid permeability wall part by EP 0645446A1 suggestion, described filter
Cylinder includes fluid intake and the fluid issuing of described fluid permeability wall portion downstream of sedimentary upstream.
The filter cylinder of this design is widely used in commercial scale processing fluid, particularly beverage, due to this
Filter cylinder can be designed accommodating more substantial granular materials and simple to operate easily.
During processing fluid, this fluid is driven through sedimentary by fluid pressure.Due to various technology
Reason, fluid pressure can not keep constant but be frequently observed the fluctuation of pressure.
The sedimentary that many useful granular materialss may rupture under the conditions of being formed at a lot, such as, more than carries
And pressure oscillation, variations in temperature or other physically or chemically affect, and produce from sedimentary upstream side to
The crack in downstream.Result no longer guarantees to flow through the homogeneous fluid stream of sedimentary, the product of the handled fluid of impact
Matter.
In order to solve this problem, it is necessary to often change sedimentary, to guarantee the reliable quality of handled fluid.
But granular materials does not the most exhaust its disposal ability.
Some granular materialss expected, as PVPP (crospolyvinylpyrrolidone) is not suitable for
This kind of filter cylinder, and it is only capable of in so-called feed proportioning system with used as stabilizers, wherein PVPP granule is fed to
In fluid and must subsequently by filter and remove.In this process, the loss of PVPP granule is substantial amounts of.
Summary of the invention
It is an object of the invention to provide a kind of method, wherein the sedimentary of granular materials can use prolongation time
Between, and allow unfavorable granular materials before use.
Above-mentioned purpose can realize by having the method for claim 1 feature.
Pending fluid is preferably liquid, more preferably such as the most above-mentioned described liquid, aqueous such as beverage.
Preferably, during sedimentary is included into the filter cylinder allowing to operate relatively easily.
The inventive process provides one uses PVPP granule as the good opportunity of granular materials, described granular material
Expect that this may use in the way of notable less economy.
Forming the risk in crack in PVPP filter cake, this crack causes pending fluid stabilized effect significantly
Degree declines, and technique will be caused uncontrollable.
Generally the most not only only one of which filter cylinder but multiple filter cylinder (each accommodate granular materials sedimentary) exist
Common housing uses, and by pending fluid feed to the fluid inlet of parallel filter cylinder.If
Forming crack in a filter cylinder, the most not only this occurs that the element forming crack must be replaced, and
It is that the most all of filter cylinder all must be replaced, in order to do not emit the process of uncontrollable fluid such as beverage
Risk.Although owing to substantial amounts of granular materials is wasted, and making such technique is to expend, but this is
Inevitably, because higher economic risk otherwise will be produced.
The invention provides a kind of method even allowing for and using this unworkable granular materials such as PVPP,
It is considered have the characteristic highly making us favor in beverage stabilisation.
The key element of the present invention is to regulate the sedimentary in filter cylinder again in the range of statement in claim 1.
According to the present invention, the key element that sedimentary regulation again processes is step:
A) sedimentary is heated to the second temperature, such as, 85 DEG C, wherein the first temperature the most about room temperature
Or it is lower；
B) after, this sedimentary being cooled to the 3rd temperature, such as, about 30 DEG C, average cooldown rate is the highest
It is of about 20 DEG C/min.
Sedimentary is heated to about 70 DEG C or higher second temperature, more preferably to about 80 DEG C or higher, has
Hereafter the advantage that sedimentary is in disinfection.In order to make sedimentary sterilize, by the second temperature preferably at 70 DEG C
Or more high maintenance about 20 minutes or more.
Preferably, before cooling step starts, this sedimentary is maintained a few minutes in the second temperature, such as,
About 5 minutes or more, preferably from about 10 minutes or more.
Although the rate of heat addition is inessential, but average cooldown rate must be carefully controlled in order to avoid exceeding previously mentioned
The upper limit of about 20 DEG C/min.
Cooling step can realize in many ways, such as by being gradually lowered temperature or by including one or many
The method that cooldown rate is altered in steps of individual step.It is preferable, however, that, any time during cooling step,
Maximum cooling rate about 20 DEG C/min should not be exceeded.Can consider according to reality and select about 0.1 DEG C/min
Value, more preferably 0.5 DEG C/min, as the lower limit of cooldown rate.
Regulation again according to the present invention processes and allows to repair sedimentary defect, because granular materials is in sedimentary
Redistributed and/or reconstructed, thus obtained the uniform treatment spreading all over whole sedimentary region.
The method of the present invention therefore allow sedimentary in filter cylinder granular materials use extend time, such as,
Must operate 6 to 12 months before being replaced at granular materials.
The method of the present invention can be carried out under the increasingly automated environment with less staff.
The most not only save the extensive work time, and often expensive granular material may be used most effectively
Material.
When just completing without any additional measures to add sedimentary by simple heating and cooling means
Heat with when being cooled to three temperature, such as, passes through externally heated filter cylinder and cooling filter cylinder to the second temperature, excellent
Gated and the fluid stream tying-in sedimentary regulated again was carried out at least part of regulation again process.
The fluid stream tying-in sedimentary regulated again is promoted and improve redistribution, and more uniformly acts on deposition
The granular materials of layer, and provide this more significant effect of regulation process again.
Applicant is not intended to be retrained by explanation below, it is believed that, it is heated to the second temperature what regulation again processed
During the step of degree, the thermal expansion of granular materials is perpendicular on the direction of fluid flow direction produce in sedimentary
Having given birth to pressure, this causes crack that may be present in sedimentary to be eliminated or close.Meanwhile, there is particulate matter
The redistribution of matter, and by carefully controlling cooling sedimentary in ground in the range of being stated in claim 1
This redistribution of granular materials, be maintained under conditions of it is subdivided cloth.
Even more preferably, then the fluid that regulates is used as coolant so that sedimentary is cooled to the 3rd temperature.Make
Allow better control over cooldown rate and cool down in a similar fashion as coolant with the fluid regulated again
Spread all over whole fluid flow cross section effective, i.e. the whole area of sedimentary.
Preferably, then regulated fluid additionally may act as sedimentary is being heated to the heating during the step of the second temperature
Mode.
It is clear that regulated fluid can circulate in sedimentary heating and cooling period again, and in the circulation time-division
Extremely and it is not cooled to desired temperature by chiller by heating devices heat.
Regulated fluid again for heating deposition layer can be differently configured from the regulated fluid again for cooling down sedimentary.
It is true that in numerous applications, one or more fluids regulated again can be selected to perform other appointing
Business, the particularly regeneration of granular materials.
In the application of beverage stabilisation, the alkalescence regulated fluid again for heating deposition layer can be equally used for solving
Inhale and remove the polyphenol adsorbed by granular materials when beverage processes, so that granular materials regeneration.?
Being heated or cooled in step subsequently, fresh water can be used as regulated fluid again, to clean alkali from sedimentary
Property regulated fluid again.Subsequently, it is possible to use acidity regulated fluid again (further) is to cool down sedimentary and
After can use with fresh water as regulated fluid again another clean, be used for drinking with final offer preparation
The sedimentary of another processing cycle of material.
Typically, before regulating startup again, fluid treatment will be interrupted.But, this is not enforceable
The process of measure and fluid even can continue when sedimentary regulates again under special case.Pending stream
Body can serve as regulated fluid again, as above narration in more detail.
If using the regulated fluid again being different from pending fluid, then before regulation again or when starting, will
Sedimentary washes pending fluid, and replaces by regulated fluid again.At the end of regulation again, then regulate
Fluid will be removed, and the sedimentary cleaned before processing pending fluid is resumed.
Most preferably by measuring adjusting again of the coolant as sedimentary downstream (as at the fluid issuing of filter cylinder)
The temperature of throttling body, controls above-mentioned cooldown rate.By measure make in week sedimentary downstream (as
The liquid outlet of filter cylinder) the temperature of regulated fluid again of coolant, it is achieved that independent of rate of flow of fluid with follow
The granular materials that the temperature contrast between regulated fluid and the actual temperature of filter cylinder again of ring and filter cylinder are accommodated
And specific heat capacity, most economical and the most accurately measure sedimentary cooling period occur temperature conditions.
As it has been described above, the rate of heat addition during the heating steps that regulation again processes is not the most crucial, but
In any case when sedimentary is heated to four temperature from the first temperature, the rate of heat addition be up to about 20 DEG C/
Minute it is preferred.In such embodiments, the 4th temperature is less than or equal to the second temperature, such as,
Lower than the second temperature about 10 DEG C.Due to reality, the lower limit of the rate of heat addition will preferably about 0.1 DEG C/minute
Clock, more preferably 0.5 DEG C/min.
In the multiple application of the application, the process of fluid includes such process, and it is based in fluid treatment
Period by from sedimentary dissolve and eluting or be allowed to inactivation and can consumable additive.In this situation
Under, it is advantageous to use again regulated fluid and in sedimentary add additive, thus recover sedimentary rise
Beginning treatment characteristic.
The present invention preferred embodiment in, sedimentary is by being existed with than granular materials by granular materials
The higher density of bulk density under dampness is filled in filter cylinder originally form, and the most more preferably loads
The initial density of sedimentary granular materials is corresponding to the bulk density under dampness being up to about 120%.From about
The loading density of 101% starts, it can be observed that significantly effect.
This measure not only provides and most preferably uses the volume provided for the filter cylinder accommodating granular materials, and
In addition the stability that sedimentary is overall, and the continuous processing phase at fluid (such as beverage) are further increased
Between granular materials being uniformly distributed in sedimentary.
According to the character of the granular materials for constituting sedimentary, even if the density of the granular materials of filling is phase
With, permeability or the fluid flow resistance of sedimentary are likely to difference.
In brewing technique, the fluid flow resistance of accumulation granule PVPP is characterized by so-called water equivalent, and water is worked as
Amount is according to Drawert, Brautechnische Analysenmethoden, Vol.III, MEBAK nineteen eighty-two
Publishing, the 658-659 page, 10.1.6.2Methode Schenk measures.
The preferred water equivalent of the PVPP granular materials sedimentary being ready to use in the inventive method is about 200
l/h*1600cm2Or more, more preferably approximately 250l/h*1600cm2Or it is more.The most about 300
l/h*1600cm2Water equivalent.
Can also ability based on Adsorption of Catechol, carry out the selection of PVPP granular materials.Stable at beverage
During change processes, use catechol as the model substance of polyphenol in such test.Preferably PVPP
Granular materials display catechol reduces about 30% or more, even more preferably about 35% or more, and when adjacent benzene
When diphenol decrement is to about 40% or more, it is contemplated that the optimum in the stabilization process of beverage.
The test that catechol reduces is carried out as follows:
80mg amount (+) catechol hydrate (Aldrich Chem Co., Milwaukee, USA) exists
It is dissolved in the ethanol of 50ml under room temperature.Catechol solution mixes with distilled water to provide 1 liter molten subsequently
Liquid S, saves it in brown bottle.
Prepared contrast solution R by 50ml ethanol, in ethanol, add distilled water to obtain 1 liter of solution.
It it is the PVPP granular materials to be measured being separately added into 50mg amount in the flask of 150ml to 4 volumes.
The catechol solution S of 100ml is joined two in these flasks.Add in remaining two flasks
Enter the contrast solution R of 100ml.
The content of flask is sufficiently mixed 5 minutes.Then, supernatant is poured in the flask of cleaning.
It is essential that be added in corresponding flask, just after 5 minutes, pour out at described whole 100ml
Supernatant.Owing to supernatant must not contain granular materials, therefore filtered by the filter of 0.45 μm.From
The supernatant (SN) that solution S obtains is referred to as SNs, and the supernatant obtained from contrast solution is referred to as SNx.
Before supernatant is carried out UV absorption detecting, it is proposed that filtered supernatant SNs and SNx will be accommodated
Flask preservation 1 hour at dark cool place.
Suggestion uses catechol in the uv absorption of 280nm, calculates PVPP with measurement with according to following equation
Absorbability, i.e. the minimizing of catechol:
Absorbability [%]=100* (E100-(Es-Ex))/E100
Wherein E100The light absorption value of=solution S
The light absorption value of Ex=contrast solution SNx
The light absorption value of Es=sample solution SNs
All of light absorption value all contrasts with contrast solution R and measures.
The parameter that catechol reduces not only describes the PVPP material activity to polyphenol, the most simultaneously by granularity
The impact of the surface area being distributed and provided by granular materials.Although due to their high surface, little granule is
Preferably, but include that the too much short grained distribution of particles of quantity will cause striding across the too high pressure of sedimentary
Power is poor.
Applying for many, granular materials mainly comprises and has about 25 μm or more
The granule of big particle diameter.
Can there is the granule less than 25 μm, and the most substantially affect by the inventive method obtained good
Effect.However, it is preferred to the amount of the granule less than 25 μm to be restricted to about 15 weight %, more preferably from about 10
Weight % or lower, even more preferably to about weight 5% or lower.
If less than the amount of quantity greater than about 15 weight % of the granule of 25 μm, too high pressure be can be observed
Difference, it makes to use this sedimentary uneconomical.
The method of the present invention particularly advantageously uses and is included in compressible in pending fluid and/or swellable
The granular materials of granule.One example of this material be PVPP in an aqueous medium.
Another kind of preferably granular materials include bead form granule and, it is further preferred that substantially by pearl shape
The granule composition of formula.Here, the commonly provided low pressure difference of particle form evenly.
Although according to many granular materialss of the present invention be likely to be used for process beverage, but granule selected from agarose,
PVPP, PA, zeolite, activated carbon and/or kieselguhr are favourable.
When layer during initial deposition is filter cylinder, compressible granule allows higher bulk density.This type
Granule provide extra benefit, because the stability of sedimentary uniformity can be enhanced again.
According to the present invention, the process of fluid covers multiple process, including preferably adsorbing, filter, attaching
Add agent (doping) and/or make the process of fluid generation chemical reaction.
The chemical reaction that the inventive method is carried out is preferably catalytic reaction, and it does not consume and is included in sedimentary
Additive, but the catalytic additive in sedimentary can use the time of prolongation during sedimentary regulates again
And/or can regenerate or supplement.
As it was previously stated, the present invention be optimum for processing aqueous fluid, preferred drink, particularly medicated beer,
Wine and fruit juice.
Preferably by using PVPP granular materials, realize beverage (particularly medicated beer, wine or fruit juice)
Stabilizing treatment.
It addition, according to the invention, it is possible to use multiple deposition layer, wherein, the most each sedimentary is included into
In separate filter cylinder, described filter cylinder provides in common housing, and the fluid that described housing has with filter cylinder enters
The parallel connected entrance of mouth and the parallel connected outlet with the fluid issuing of filter cylinder.
Preferably, the multiple deposition layer in these filter cylinders provides in the form of a laminate, and described lamination is more preferably
It is orientated in vertical direction.
When multiple filter cylinder is contained in and has in the common housing of fluid intake and fluid issuing, such
In embodiment, average cooldown rate is preferably by measuring the temperature of the exit regulated fluid again of common housing
And determine.
When using this lamination, then the heating steps that regulation processes preferably passes through regulated fluid again from housing
Bottom end introduces to be implemented in housing.
Then cooling step is preferably by implementing regulated fluid again from the top end introducing lamination of lamination.
Hereinafter, various aspects of the invention and advantage will be explained in greater detail in conjunction with corresponding drawings and Examples.
Brief Description Of Drawings
In the accompanying drawings
The schematic diagram of the equipment that accompanying drawing 1 display processes for the regulation again performing the present invention；
Accompanying drawing 2A and B shows the example filter being contained in the granular materials sedimentary used in the inventive method
The details of cylinder；
Accompanying drawing 3 display is for being fed to granular materials in multiple filter cylinder form the exemplary device of sedimentary；
Accompanying drawing 4A, B and C show the deposition accommodating initial, fracture and the particulate matter of adjustment state more respectively
The filter cylinder of layer；
Accompanying drawing 4D shows the diagram of various parameters during sedimentary of the present invention regulates again；
Accompanying drawing 5 represents the gratifying distribution of particles of the granular materials being ready to use in the inventive method；With
Accompanying drawing 6 display introduces the diagram of the fluid handling system of the inventive method.
Detailed Description Of The Invention
Accompanying drawing 1 display is for carrying out the diagram of the configuration 10 of the critical process of the inventive method, say, that
Through being used for processing the granular materials sedimentary of fluid (such as, such as the beverage of medicated beer, wine or fruit juice)
Regulation processes again.
Configuration 10 includes that the housing 12 accommodating filter cylinder 14, the layer of granular materials (not having display) are sunk
Amass in this filter cylinder.Housing 12 is included in the fluid intake 16 at its top and the fluid issuing 18 bottom it.
Of course, it is possible to provide the housing 12 of large-size, in order to it can accommodate the lamination of multiple filter cylinder 14.
Fluid intake 16 is connected with pipeline 20, and it provides from entrance 16 to pump 22 (such as, fluid-control
Centrifugal pump) fluid flow path,.
Pipeline 20 is advantageously equipped with effusion meter 24, temperature sensor 26 and pressure transducer 28, and they allow
Monitor via the granular materials sedimentary upstream side accommodated in pump 22 and pipeline 20 to entrance 16 and filter cylinder 14
The temperature of fluid, pressure and flow velocity.
Outlet 18 is connected with the pipeline 30 leading to heat exchanger 32, and described heat exchanger 32 is via pipeline 34
It is connected with the entrance of pump 22, thus forms closed-loop path.
The pipeline 30 of connection outlet 18 and heat exchanger 32 is equipped with temperature sensor 36 and pressure transducer
38, they allow monitoring to circulate downstream pressure and the downstream temperature of the regulated fluid again flowing through filter cylinder 14.
During once filter cylinder 14 is placed in housing 12, housing just Guan Bi, and by pump 22, pipeline 20, have
The closed-loop path that the housing 12 of filter cylinder 14, pipeline 30 and heat exchanger 32 and pipe 34 are constituted is regulated stream again
Body is full of, this again regulated fluid there is the temperature of rising preferably via valve V1.
Pipeline 20 includes an arm 40 near entrance 16, and this arm can connect pipeline 20 and entrance
16 or close via valve V5.In the upstream of arm 40, pipeline 20 includes shutoff valve V3 and can be via
Another arm 42 that valve V4 is connected with pipeline 20.
Pipeline 30 can be closed via valve V7.In the upstream of valve V7, pipeline 30 can be via shutoff valve
V6 is connected with arm 44.
When filling hot water to closed-loop path, when regulating beginning again, open valve V1, V3, V4 and V5,
To discharge the air accommodated in the closed circuit, when valve V6 opens, the regulated fluid more originally measured can
Discharge via arm 44.Subsequently, opening valve V7, closed-loop path is filled completely.Valve V4 and V5
To be closed, the heating steps by carrying again regulated fluid sedimentary in cartridge filter 14 can be started.
During the initial period of heating steps, valve V6 can keep open to discharge a part of recirculation again
Regulated fluid, this again regulated fluid provided to the fresh fluid in loop via valve V1 and replaced.This mistake
Journey allows the fluid that regulates again of discharge part, its when the beginning that sedimentary regulates again can in a large number load from filter cylinder
The material of the granular materials desorbing in 14.
Hereafter, valve V1, V2, V5 and V6 keep or are closed, and valve V3 and V7 is open.
Situation when regulated fluid again leaves housing 12 monitored by pressure and temperature sensor 36 and 38.Then flow
Body is transported in heat exchanger 32, and here fluid is heated to the temperature preset again.
In order to reach this effect, heat exchanger is via valve VVL2 and VRL2 and heater (not shown)
Connect, with by heat exchanger 32 and its heat exchanging pipe 33 circulating-heating medium (such as, hot water).
Once temperature sensor 36 shows that sedimentary has been heated to target the second temperature, valve VVL2 and VRL2
With regard to final plant closure and open the most again, be maintained the second temperature with the temperature by regulated fluid again.
After the preset lime, this time preferably ensures that sedimentary is in aseptic condition, is connected by heat exchanger
In chiller (not shown) and open valve VVL1 and VRL1 so that cooling medium cycles through heat exchange
The heat exchanging pipe 33 of device 32.
Subsequently, the regulated fluid again of cooling by pump 22, pipeline 20, have filter cylinder 14 housing 12, pipe
The closed-loop path that road 30, heat exchanger 32 and pipeline 34 are constituted is circulated.Cooldown rate is via temperature sensing
Device 26 is monitored.
In addition the cooldown rate of sedimentary is by the temperature being connected with the pipeline 30 near the outlet 18 of housing 12
Degree sensor 36 is monitored.This temperature sensor 36 shows the cooldown rate of sedimentary in filter cylinder 14.
Accompanying drawing 2 shows the example filter cylinder for accommodating granular materials sedimentary used according to the inventive method.
Accompanying drawing 2A represents the upward view of filter cylinder 14, and this filter cylinder has the bottom of a substantially fluid-tight for dish type
Wall 60, it has the central opening 62 being provided with central hub 64.
In the periphery of base wall 60, it is connected to sidewall 66, such as, connects with welding step.
Sidewall 66 is looped around the whole periphery of base wall 60, in order to limit the granule accommodating sedimentary form
The chamber 70 of material.
The bottom of chamber 70 is covered by Web materials 72, and described Web materials 72 has sufficiently small retaining
The granular materials of sedimentary, and for pending fluid and the one that used is regulated again for sedimentary
In any case or be all the opening of permeability for multiple fluid.
Web materials 72 covers substantially all of base wall 60 and extends to central opening 62.When the end of at
When installing wheel hub 64 on portion's wall 60, Web materials 72 is clipped between wheel hub 64 and base wall 60, thus permits
The ejection being permitted chamber 70 enters the centre gangway that wheel hub 64 is limited.
If this filter cylinder is filled and operates at horizontal level, the top surface of filter cylinder 14 just can keep open.By
In actual reason, preferably close the top of filter cylinder 14, this dish by the pan-shaped cover prepared by Web materials 76
Shape lid is fixed on sidewall 66, such as, by welding, in order to close the upper end of chamber 70 and by particulate matter
It is trapped in chamber 70.Web materials 76 is connected to the top half of wheel hub 64 to avoid fluid from chamber
The top of 70 is fed directly in the centre gangway of wheel hub 64.Web materials 76 can be to connect movably
Receive sidewall 66 and wheel hub 64.
The sidewall 66 of filter cylinder 14 is provided with entrance 80, and once the chamber 70 of filter cylinder 14 granular materials is filled extremely
Desired degree, this entrance is just closed by bolt 82.
Central hub 64 not only serves as the outlet of filter cylinder 14, and is also used for fixing at filter cylinder 14 middle body
Web materials 72 and 76.It addition, can surface and bottom surface section be designed on which, in order to when filter cylinder that
This stacked on top with formed as above the most-filter cylinder lamination time, accommodate corresponding filter cylinder.
Although filter cylinder 14 and each parts thereof can be by metal manufactures can be with the granular materials being replaced in chamber 70
And be recycled for multiple times, it is also contemplated that being manufactured filter cylinder 14 by plastic components, it is disposably filled and is made
It is dropped together with the granular materials consumed at the end of life cycle.
The size of filter cylinder used in example described in the invention has the internal diameter of about 540mm and about 30mm's
Packed height, the internal diameter of wheel hub 64 is about 65mm, and the external diameter of wheel hub is about 116mm.This filter cylinder is provided
Chamber 70 amount to 6.5 liters.
The diagram of accompanying drawing 3 display configuration 100, this configuration can be simultaneously used to fill multiple filter with granular materials
Cylinder 14.
To this end, configuration 100 includes being equipped with entrance 104 at an upper portion thereof and being equipped with outlet 106 bottom it
Tank 102.Additionally, in the bottom of tank 102, it is provided that agitator 108, it allows the content of agitator tank 102
Thing, such as, the granular materials suspended substance in filter cylinder 14 to be filled.
Filter cylinder 14 is placed with stand up position and is connected to fill pipe 110 by their entrance opening 80, should
Fill pipe and be contained in the suspended substance in tank 102 via centrifugal pump 112 reception.
Fill pipe 110 and be equipped with one or more pressure transducer, in order to monitoring is during the filling of filter cylinder 14
Inlet pressure.The inlet pressure monitored by sensor 112 determines the filling journey of granular materials in filter cylinder 14
Degree.
If using the granular materials such as PVPP of swellable, then initially allow for granule and absorb fluid around, example
As, water.For PVPP granule, the swelling time of about 4 hours is enough, and more preferably from about 10 is little
Time swelling time.Suspension preferably comprises the PVPP granule of about 2 to 10 weight %, and more preferably from about 3 to about
The PVPP granule of 5 weight %.Subsequently this suspension is stirred in tank 102, then by centrifugal pump 112
In the loop with flow velocity about 4m3/ h circulates about 15 minutes, and is not filled with filter cylinder.Depend on granular materials and institute
Use is specific the most standby, can advise carrying out flow velocity fine setting, to avoid deposition and/or the classification of granule in the loop.
Subsequently, filter cylinder can be connected with loop via ball valve 118 and feeding line 120.
When starting to fill filter cylinder 14, the fluid of suspended particle material is via their roof 76 and wheel hub 64
And leave filter cylinder 14.Filter cylinder 14 is after filling continuously, and the Fluid Volume leaving filter cylinder 14 tails off, until
The latter stage of filling process, when having produced certain bolt of granular materials at the entrance 80 of filter cylinder 14, closely
Like stopping.
Filling the downstream of pipe, provide valve 116 in the loop, it can be used for regulating filling pipe 110
Or the stuffing pressure that several position is sensed.Pressure transducer 112 shows the stuffing pressure of filter cylinder 14, measures
The filling extent of single filter cylinder or filling.Preferably, the pressure differential being used for filling filter cylinder 14 is about 0.3 bar.
It is essential that fill filter cylinder with granular materials tight ground.
For the filter cylinder 14 of the chamber 70 with about 6.5 liters as shown in Figure 2, the typical filling time can
In the range of about 20 to about 30 minutes.
Then being disconnected with filling pipe 110 by filter cylinder 14, the entrance 80 of filter cylinder 14 sidewall 66 is by blind
Bolt 82 and close.
When needing precompressed PVPP layer in filter cylinder 14, preferably PVPP and a certain amount of water-soluble
Packing material is filled in filter cylinder 14 in the dry state.Flow through filter cylinder making current and wash out filling material
After material, PVPP granule by swelling and in filter cylinder 14 produce precommpression filter cake.As water soluble filler materials,
Particularly food compatible material, such as, salt and sugar can be used.
Swelling effect in view of the about 1.4 times of dry volumes obtained with PVPP, it is necessary to calculate amount of filler to keep away
Exempt from the unacceptable excessive filling of filter cylinder 14 or excessively load, and (i.e. filter cylinder 14 exists in following steps
Application in stabilisation beverage) period produce excess pressure poor.
Suggestion carries out some laboratory scale pretest, to find out the certain filling treating to mix with PVPP granule
Material optimized percentage.
Accompanying drawing 4A display top Web materials 76 be removed after filling filter cylinder 14, and rising in filter cylinder 14
Beginning sedimentary 140 demonstrates smooth surface.
In order to prove sedimentary regulate again after the effect of the present invention, PVPP particulate matter the layer prepared is the most such as
Spontaneous breaking as being described below.
After filling filter cylinder 14, the sedimentary obtained has been passed through repeatedly the flowing of start-stop fluid and has been followed
Ring and spontaneous breaking, and damage (seeing accompanying drawing 4B) by introducing compressed air in addition.Sedimentary 140
Showing multiple serious crack 142, it is constituted from the upstream face of layer 140 to filter cylinder Web materials 72 (i.e.
The downstream surface of sedimentary) shortcut.
Hereafter, following condition is stood including the filter cylinder 14 of sedimentary 140 damaged:
The top of filter cylinder 14 as shown in fig. 4b is equipped with the lid of Web materials 76.Subsequently filter cylinder is installed
In the housing 12 of accompanying drawing 1 regulating allocation 10 again, and close this housing.
In initial step, then the cold water that regulating allocation temperature is 2 DEG C is filled, and is equivalent to usual beverage such as beer
The first temperature that wine is stabilized.Recirculation of cold water about 10 minutes is to determine the pressure differential of faulted deposit layer.?
The value of the pressure differential recorded when 2 DEG C is 0.73 bar, and the flow of cold water is 0.59m3/h。
Hereafter, the temperature of recirculation water raises further with the speed of about 6 DEG C/min, until housing 12 exports
Temperature be about 70 DEG C (being recorded by temperature sensor 36) (the 4th temperature).Flow velocity is at 0.59m3/ h protects
Hold constant.
Temperature is increased to the second temperature 85 DEG C further with the speed being gradually lowered.80 DEG C or higher temperature
Under, at the 0.59m of recirculation water3Under the most identical flow of/h, the process of sedimentary the most about 20 minutes.
Subsequently sedimentary is cooled to the controlled cooldown rate of about 5.5 DEG C/min the 3rd temperature of about 20 DEG C.
Accompanying drawing 4D illustrates the parameter measured during said process: temperature (curve A), flow are (bent
Line B) and pressure differential (curve C),.
Accompanying drawing 4D proves, during above-mentioned regulation again, by the pressure differential (curve C) of observation, to occur in deposition
Change in Rotating fields is considerably advantageous:
During making first step of recirculation of cold water in the closed-loop path of configuration 10, pressure differential is in a few minutes
Within reach the plateau value of 0.73 bar.After sedimentary 140 in heating filter cylinder 14, granule PVPP material
Expand swollen, cause the most closely knit structure, and pressure differential drops to about 0.15 bar.
Sedimentary 140 is after controlled cooling, and its structure again becomes more closely knit and pressure differential and grows steadily
To 0.77 bar or higher level, i.e. be significantly higher than originally to the value (0.73 measured by faulted deposit layer
Bar), the reparation in display crack 142.
When being removed and eliminate netted lid 76 from housing 12 by filter cylinder, then the sedimentary 140 regulated can
With by visual assessment.As shown in accompanying drawing 4C, serious crack is repaired, and the most residual at layer 140 top
Little apparent irregular 144 stayed do not affect the performance of stabilisation.
The most serious granular materials sedimentary as shown in fig. 4b is destroyed and is not generally occurred at fluid treatment
In practice.Therefore, the test result obtained ensure that, is occurred during regularly fluid treatment circulates
Any destruction can be repaired during present invention regulation process again.
The granular materials having been described above being explained in detail in selecting being suitable for forming the sedimentary in filter cylinder 14
Importance.
For PVPP, the typical granularity of the PVPP reproducible food-grade particles material being obtained commercially is divided
Cloth is shown as curve A in figure 5, and it is relatively wide and includes substantial amounts of little granule.
At one or many, commercially available initial PVPP granular materials is suspended in about 5 weight % amounts
In water, and poured out supernatant at about 4 hours after time of repose, it is possible to obtain according to the granularity of curve B
Distribution.Compared with the distribution of particles according to curve A, demonstrate that pressure drop is notable according to the distribution of particles of curve B
The behavior improved.
Other distribution of particles that can work very well confirms in curve C and D, according to the distribution of particles of curve C
Than the granular materials corresponding to curve B and D, there is slightly higher small particle content.
The granular materials of different sample B, C and D can be further characterized by the parameter included in table 1.
Table 1
| Sample | The part [volume %] of particle diameter ＜ 25 μm | d10Value | d50Value | d90Value |
| Curve B | 6.2 | 44.6μm | 104.9μm | 239.0μm |
| Curve C | 1.38 | 39.6μm | 91.3μm | 204.6μm |
| Curve D | 2.03 | 45.4μm | 108.6μm | 244.2μm |
Accompanying drawing 6 illustrate for beverage, particularly medicated beer process configuration 200 schematic diagram, its for from
Medicated beer is removed polyphenol, and its granular materials also allowing for being used in absorption and removal polyphenol regenerates and adjusts
Joint.
Configuration 200 includes the cylindrical housings 202 accommodating the lamination 204 of filter cylinder 14, their center hub
Part 64 aligns to form continuous print passage 206.
About as described in accompanying drawing 3, filled filter cylinder 14 with PVPP granular materials.The particle diameter distribution of PVPP material
Similar to what curve B in accompanying drawing 5 showed.
Housing 202 has top and movably covers 208, and it includes fluid intake 210, beverage to be stabilized
Imported in housing 202 by it.
Beverage is then filled with all volumes of housing 202, and via the meshy surface on each filter cylinder each top
76 (seeing accompanying drawing 2B) enter in each parallel filter cylinder 14, subsequently into the deposition of granule PVPP material
In Ceng, and leave filter cylinder 14 via lamina reticularis 72 and leave via the outlet 212 bottom housing 202
Central hub 64 and passage 206.Medicated beer is fed to configure 200 and via medicated beer via beer inlet 214
Configuration 200 is left in outlet 216.
In order to provide continuous print medicated beer stream, using centrifugal pump 218, it is respectively via pressure and flow transducer
220 and 222 control pressure and flow velocity.The temperature of medicated beer is generally within the scope of 0 DEG C to about 10 DEG C and be considered as
First temperature.
When leaving container via outlet 212, monitored the pressure of the medicated beer of stabilisation by pressure transducer 224
Power.
During the stabilizing treatment of medicated beer, remaining of configuration 200 is the most standby keeps inoperative.
After about 6 to 10 hours, the capacity being included in the granular materials in filter cylinder 14 has exhausted, and needs
The regeneration of granular materials to be carried out.
Regeneration step is the most respectively by the fluid by alkalescence with acidity, such as, NaOH aqueous solution and HNO3Water
Solution rinses filter cylinder 14 and the sedimentary wherein accommodated is carried out.
In the first regeneration step, lamination and housing 202 with water rinsing filter cylinder 14 are to remove the medicated beer of residual.
Afterwards, by making the water being contained in configuration 200 circulate, filter cylinder 14 is heated to the second temperature 85 DEG C.
Determine that the second temperature is 85 DEG C, in order to before the lamination of filter cylinder 14 is filled with medicated beer to be stabilized again,
The sterilizing of the pipeline of filter cylinder and their sedimentary and housing 202 and configuration 200 is provided.
Can to for making the technique of the granule PVPP material regeneration being contained in filter cylinder 14 improve, with
Reach regulating again the sedimentary in the filter cylinder 14 according to the present invention, thus formed in sedimentary the most at last
Crack or other destroys or distribution of particles inhomogeneities is repaired, thus the sedimentary of PVPP granular materials is again
It is in the state (see accompanying drawing 4C) the most suitable with during initial filling.
In order to provide the heating smoothly of granular materials in filter cylinder 14, control recirculation by heat exchanger 226
The temperature of water, in order to they are higher 20 to 30 DEG C than housing 202 outlet temperature (temperature sensor 228).
Control the flow of hot water so that temperature per minute raises about 5 to 7 DEG C.
In circulating water heating and housing 202 during the heating of filter cylinder 14 lamination or the second temperature 85 DEG C
After reaching, sodium hydroxide is fed in recirculation water from reservoir 230 by feed pump 232, until
Obtain the concentration of 1 weight %.
The water comprising 1 weight % sodium hydroxide is circulated continuously 10 minutes, during this period, via arm 240
With valve 242, sodium hydroxide medium discharged configuration 200, in order to remove the solution being included in sodium hydroxide solution
The polyphenol inhaled.Via valve 236, by discharge regulate again/regenerative fluid part water reservoir 234 in new
Fresh water replaces.The hot water of the sodium hydroxide that then will contain from about 1 weight % amount (closes valve in the closed circuit
236 and 242) other 20 minutes of recirculation.
Hereafter, completing to remove the polyphenol previously adsorbed from granule PVPP material, alkaline fluids is via pipeline
240 and valve 242 from configuration 200 discharge and by from water reservoir 234 fresh hot water replace, when passing through
During heat exchanger 226, the freshest hot water is heated to the temperature identical with the alkaline matter of previous recirculation
Degree.Rinse in configuration 200 with fresh water until leaving the electrical conductivity of water of housing 202 less than 0.5mS.
Hereafter, lamination and the cooling of sedimentary therein of the careful filter cylinder 14 controlled are started.According to the present invention,
The most important thing is, cooling step is carried out at a temperature of closely controlling, thus does not has temperature jump to put on filter
Sedimentary in cylinder 14, in order to keep their integrity.
Herein, the recirculation flow temperature that the temperature of entrance is controlled in than housing 202 exports at 212 is low about
10 to 15 DEG C.Heat exchanger 226 runs as chiller now.
Meanwhile, can be by acid, such as, HNO3, add to from the loop of reservoir 238 and feed pump 232 until
In recirculation water, the amount of acid reaches about 0.5 weight %.
During the recirculation of acid water, the 3rd temperature maintains the level of 20 to 25 DEG C.
This process then passes through cold water (from water reservoir 234) and cleans extra 3 minute, and the effect of cleaning is led to
Cross measurement electrical conductivity of water and control, until the upper limit that electrical conductivity of water is less than 0.5mS.
The temperature of the fluid for cleaning may remain in about 20 DEG C.
At the completion of this step, the lamination of filter cylinder 14 and their sedimentary are suitable for the beverage such as medicated beer
The new circulation of stabilisation.
Said process this have the advantage that, filter cylinder 14 and PVPP material deposits is positively retained in housing 202,
And stabilisation medicated beer can be reused for immediately.
Equally, the polyphenol substance that adsorbed by desorbing in alkaline fluids environment and regenerate granular materials and led to
The time often needed, heating deposition layer simultaneously can be used for, thus process granular material for desorbing polyphenol
Granule in material and heating deposition layer regulates can realize simultaneously for it.Equally, can realize cleaning simultaneously
Filter cylinder and sedimentary therein and cooling thereof, thus can be incorporated into that the most steady according to the regulation again of the present invention
The typical regeneration process carried out during fixedization.
Claims (24)
1., for the method processing fluid, described method includes:
The granular materials of the sedimentary form with upstream side and downstream is provided；
Starting the process of described fluid, it is by guiding described fluid at the first temperature from described sedimentary
Upstream side flow to the downstream what side was carried out；
Regulating again of described sedimentary；
The process again of described fluid is carried out by guiding described fluid to flow through the sedimentary regulated again；
Wherein said regulation again includes step
-sedimentary is heated to the second temperature；With
-sedimentary is cooled to the 3rd temperature, average cooldown rate in the range of the highest 20 DEG C/min, its
In any time during cooling step, maximum cooling rate 20 DEG C/min should not be exceeded.
Method the most according to claim 1, wherein said fluid is beverage.
Method the most according to claim 2, wherein said beverage is medicated beer, wine or fruit juice.
4. described in the process of claim 1 wherein, regulation includes guiding again regulated fluid to flow through sedimentary again.
5. the method for claim 4, wherein said regulated fluid again is used as during the step of cooling sedimentary
Coolant, the described optional recycle of regulated fluid again passes through chiller.
6. the method for claim 5, wherein leaves sedimentary downstream using the regulated fluid again as coolant
Temperature determine cooldown rate.
7. the method any one of claim 4 to 6, wherein when being heated to described second temperature, described
Again regulated fluid be used as sedimentary add thermal medium, the described optional recycle of regulated fluid again passes through heater.
8. the method any one of claim 1 to 6, wherein the regulation again of sedimentary additive is included in heavy
Lamination.
9. the method any one of claim 1 to 6, wherein said sedimentary is by by described granular materials
Being filled in filter cylinder be formed, described granular materials has the bulk density than the granular materials under dampness
High density.
Method the most according to claim 9, wherein the initial density of the granular materials of sedimentary filling is equivalent to
The bulk density under dampness of at most 120%.
11. methods according to claim 10, wherein said initial density is 101% or higher at moist shape
The bulk density of the granular materials under state.
Method any one of 12. claim 1 to 6, wherein the particle diameter included by granular materials is less than 25
The amount of the granule of μm is 15 weight % or lower.
Method any one of 13. claim 1 to 6, wherein granular materials is included in pending fluid
The granule of middle swellable.
Method any one of 14. claim 1 to 6, wherein said granular materials includes bead form
Granule.
Method any one of 15. claim 1 to 6, wherein granular materials include selected from agarose, PVPP,
PA, zeolite, activated carbon and/or diatomaceous granule.
Method any one of 16. claim 1 to 6, wherein the granule of granular materials is selected from compressibility
Granule.
Method any one of 17. claim 1 to 6, wherein said process includes adsorbing, filters, adds
Additive and/or make fluid react.
18. methods according to claim 17, wherein said reaction is catalytic reaction.
Method any one of 19. claim 1 to 6, wherein multiple deposition layer carries in common housing
Confession, this housing has the entrance that the upstream side with sedimentary is connected and the outlet being connected with the downstream of sedimentary.
The method of 20. claim 19, includes in each sedimentary in separate filter cylinder.
The method of 21. claim 20, described filter cylinder provides in the form of a laminate.
The method of 22. claim 21, the lamination of described filter cylinder is contained in described common housing.
The method of 23. claim 22, described lamination in the vertical direction is orientated.
Method described in 24. claim 19, wherein in described heating steps, when heating deposition layer,
By regulated fluid again in housing bottom introduces housing and/or wherein in described cooling step, will regulate again
Fluid introduces housing from the top of housing.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP10169583.1 | 2010-07-14 | ||
| EP10169583.1A EP2407530B1 (en) | 2010-07-14 | 2010-07-14 | Method for treating a fluid, in particular a beverage |
Publications (2)
| Publication Number | Publication Date |
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| CN102391942A CN102391942A (en) | 2012-03-28 |
| CN102391942B true CN102391942B (en) | 2016-08-17 |
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| US (1) | US9670441B2 (en) |
| EP (1) | EP2407530B1 (en) |
| JP (1) | JP5909834B2 (en) |
| KR (1) | KR101872200B1 (en) |
| CN (1) | CN102391942B (en) |
| AU (1) | AU2011204776B2 (en) |
| BR (1) | BRPI1103237B1 (en) |
| CA (1) | CA2746113C (en) |
| DK (1) | DK2407530T3 (en) |
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| CN103118543B (en) * | 2010-09-07 | 2015-01-14 | 皇家飞利浦电子股份有限公司 | Coagulant control for producing tofu |
| CN103525604B (en) * | 2012-07-03 | 2014-12-31 | 郑海鸿 | Beer beverage and preparation method thereof |
| KR101349048B1 (en) * | 2013-06-13 | 2014-01-10 | (주)경원산업 | Drinking-water manufacturing device and control method for disorder in it |
| AU2014355200B2 (en) * | 2013-11-28 | 2018-09-20 | Cytiva Bioprocess R&D Ab | Stabilization of fermented beverages |
| US10512701B2 (en) | 2015-08-28 | 2019-12-24 | Michael Papadopoulos | System for fluid sterilization for a vessel |
| NZ740103A (en) * | 2015-08-28 | 2019-06-28 | Michael Papadopoulos | System and method for fluid sterilization |
| KR101838967B1 (en) | 2015-10-08 | 2018-03-15 | 엘지전자 주식회사 | Convenience Apparatus for Vehicle and Vehicle |
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| DE10217262A1 (en) * | 2002-04-18 | 2003-11-06 | Pall Corp | Filter module and method for producing a filled filter module |
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2010
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| JP2012019785A (en) | 2012-02-02 |
| US9670441B2 (en) | 2017-06-06 |
| CN102391942A (en) | 2012-03-28 |
| KR20120007450A (en) | 2012-01-20 |
| EP2407530A1 (en) | 2012-01-18 |
| AU2011204776B2 (en) | 2016-01-28 |
| JP5909834B2 (en) | 2016-04-27 |
| KR101872200B1 (en) | 2018-06-28 |
| AU2011204776A1 (en) | 2012-02-02 |
| ES2426602T3 (en) | 2013-10-24 |
| EP2407530B1 (en) | 2013-08-21 |
| MX2011007488A (en) | 2012-01-17 |
| CA2746113A1 (en) | 2012-01-14 |
| BRPI1103237B1 (en) | 2019-11-19 |
| US20120015086A1 (en) | 2012-01-19 |
| BRPI1103237A2 (en) | 2013-04-16 |
| CA2746113C (en) | 2015-03-17 |
| SG177837A1 (en) | 2012-02-28 |
| DK2407530T3 (en) | 2013-10-28 |
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